Method using gaschromatographic mass spectrometry to determine lead tetraethyl in environmental water sample
A technology of gas chromatography mass spectrometry and tetraethyl lead, which is applied in the detection of environmental water samples and the field of determination of tetraethyl lead in environmental water samples by gas chromatography mass spectrometry, can solve the problems of inability to meet the actual detection requirements, serious environmental pollution and cumbersome operation and other problems, to achieve simple operation, reduce environmental pollution, and good repeatability
Inactive Publication Date: 2019-03-29
嘉兴华才检测技术有限公司
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Problems solved by technology
According to the standard requirements, the analysis of tetraethyl lead is recommended to be determined by the dithizone colorimetric method in the "Hygienic Standards for Drinking Water Quality", but this method needs to use highly volatile pure bromine and highly toxic reagent potassium cyanide. It is cumbersome and seriously pollutes the environment, and cannot meet the actual testing requirements
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[0019] A kind of gas chromatography mass spectrometry of the present invention measures tetraethyl lead in environmental water sample, comprises the following steps:
[0020] a) Take 200mL water sample, add NaCl: 20g and stir until completely dissolved to obtain pretreated water sample, sodium chloride is superior pure sodium chloride;
[0021] b) Add 50mL of n-hexane to the pretreated water sample, oscillate fully, let stand to separate layers, take the n-hexane layer, remove water through anhydrous sodium sulfate, concentrate, and dilute to 1mL to obtain a constant volume solution, and the oscillator is at a constant temperature Oscillator, the rotation speed is set to 175rpm, and the oscillation time is 60min;
[0022] c) Take 1 μL of constant volume solution and analyze it through the analyzer.
[0023] standard curve line
[0024] Accurately measure different volumes of tetraethyl lead standard solutions, dilute them with n-hexane, prepare tetraethyl lead standard worki...
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The invention discloses a method using gaschromatographic mass spectrometry to determine lead tetraethyl in an environmental water sample. The method comprises the steps that a) the water sample of 200 is taken, added into NaCl: 20 g and stirred until complete dissolution to acquire a pretreated water sample; b) n-hexane of 50 mL is added into the pretreated water sample; sufficient shaking and standing for stratification are carried out; an n-hexane layer is taken; water is removed by anhydrous sodium sulfate; concentrating and diluting to 1 mL to acquire a constant volume solution; and c) the constant volume solution of 1 mu L is taken and analyzed by an analysis machine. The method provided by the invention has the advantages of simple operation, reduced environmental pollution, wide detection linear range, good repeatability and accurate quantitation, and fully meets the requirement of stipulated detection lower limit of lead tetraethyl in the water quality standard.
Description
【Technical field】 [0001] The invention relates to the technical field of environmental water sample detection, in particular to the technical field of measuring tetraethyl lead in environmental water samples by gas chromatography mass spectrometry. 【Background technique】 [0002] Tetraethyl lead is a severe nerve poison. Due to its strong fat solubility and volatility, it decomposes when it meets water or heat to release toxic and corrosive gases. Tetraethyl lead in the environment is gradually degraded into triethyl lead by the action of light and heat, and then further degraded into inorganic lead. The poisoning symptoms of tetraethyl lead are different from those of inorganic lead, and the symptoms of central nervous system are the most intense. The initial symptoms of poisoning include sleep disturbance, general weakness, emotional instability, autonomic dysfunction, etc., often with decreased blood pressure, body temperature, and pulse rate. In severe cases, toxic enc...
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IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14
Inventor 斯广杰孙海涛孙能惠孙轶周晓佳严丽娟
Owner 嘉兴华才检测技术有限公司